Apparatus for the treatment of mineral oils



June 11, 1929. w. F. DOWNS APPARATUS FOR THE TREATMENT OF MINERAL OILS Filed Nov. 24, 1922 2 Sheets-Sheet 3.

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' June 11, 1929. w, 7:, owns 1,716,372

APPARATUS FOR THE TREATMENT OF MINERAL OILS Filed Nov. 24, 1922 2 Sheets-Sheet 2 YIIIIIIIIIIIIIIIIIIIIIII/IIIIIIIII I llu Patented June 11, 1 929.

,UNITED'STA'TES PATENT OFFICE.

WILLIAM F. DOWNS, or CHATHAM, NEW JERSEY; MARY GARDNER DOWNS ADMINIS- zrna'rnrx or sans WILLIAM F. nowns-nncmsnn.

APPARATUS FOR THE TREATMENT OF MINERAL OILS.

Application filed November 24, 1922. Serial No. 602,933.

5 pounds, and increase the percentage of compounds of lower boiling point, but it has heretofore been considered that commercially satisfactory results could be obtained only by the application of heat to the mixture of the mineral oil and aluminum chloride.

I have discovered that such heat treatment is not essential, particularly where the improvement sought is in .regard to color, odor and saturated condition of the molecules. One object of my present invention is to secure such improvement in a commercially practical manner at ordinary room temperatures. My invention involves a novel method of securing this result under these conditions.

The aluminum chloride has the property of attracting to itself heavy tar-like, highly carbonaceous compounds. When employed with an oil in which such heavier or high boiling point hydrocarbons are dissolved,or blended, the aluminum chloride draws these heavier compounds to itself and thereby detars and decolors the mixture of oil. The heavy material which assembles about the chloride is no longer miscible in the oils from which it has been withdrawn and forms agglomerations with the aluminum chloride particles as nuclei, which readily settle to the bottom of the container. As soon as any portion of the chloride becomes enveloped in the tarry matter its power is diminished, and when the envelope is sufficiently thick the chloride becomes inert. Although heating of the mixture particularly to a temperature above the volatilizing point of the aluminum chloride tends tobreak up such agglomerations or increase the activity of the aluminum chloride, I have discovered that I canmaintain the active condition and cause the operation to that fresh surfaces of the aluminum chloride are continually exposed for direct action on the oil. Any ordinary agitation merely serves to distribute the separated agglomerates throughout the liquid and does not accomplish the desired mechanical disrupting action which constitutes a feature of my invention.

- As a further feature of my invention, I subject the oil to a two-step treatment, whereby the tarry bodies are first separated and thereafter the resulting liquid is subjected to the action of aluminum chloride in the absence of such tarry bodies, to effect a conversion of the unsaturated compounds into saturates.

The treatment of mineral oil at room tem per-ature is particularly applicable to gasoline, kerosene, lubricatmg oil, or other hydrocarbons. Where the prime object is to improve the color, odor and condition of saturation. The oil and aluminum chloride mixture may be mechanically treated so as to continually disrupt the agglomerations may be heated to its boiling point, or at least to the point at which vapors are rapidly evolved, while the liquid in the still or other vessel is'being mechanically treated as heretofore indicated. The vapors together with such portion of the vaporized aluminum; chloride as may enter the outlet from the still, pass over to a condensing chamber through a passage maintained at a temperature above that at which the aluminum chloride will condense and accumulate, so'that none of the latter accumulates in the passage to obstruct the outlet of the still. The condensing chamber includes a filter bed maintained at a temperature below the vaporizing point of the aluminum chloride so that such aluminum chloride as is carried off with the 011 vapors will here condense and the 011 vapors or the condensed liquid will be caused filtering chamber maintains its activity for.

a long period of time without replenishing and without such disrupting action'as is carried on in the still, although it may be stirred up from time to time if necessary or desirable. I

In the accompanying drawings I ha-ve illustrated a form of apparatuswhich may be employed for carrying out my improved process, and which itself forms a portion of my invention. In these drawings:

Fig. 1 is a central vertical section.

Fig. 2 is a top plan View.

Figs. 3, 4 and 5 are sections on the lines 33, 44 and 5-5 respectively of Fig. 1, and v 1 f Fig. 6 is a section similar to a portion of Fig. 1, but showing an alternative form.

In the construction illustrated there is provided a chamber 10 of suitable size and material for the treatment of themineral oil with the aluminum chloride. Vithin the chamber there is provided a beater having blades which coact to effect a breaking up of the agglomerated masses resulting from the accumulation of tarry matter on the aluminum chloride particles. ,The beater blades are illustrated as two frames or loops 11 mounted on parallel shafts 12 and 13 mounted for rotation in opposite directions, and with the blades or loops each intersecting the path of the other. During the rota-' tion the blades pass closely adjacent to each other and effect a cutting or breaking up of the masses. Any suitable means may be employed for rotating them, but as shown they are provided with meshing gears 14 and 15 of the same pitch diameter, and one shaft is provided with means, such for instance as a belt pulley 16, whereby power may be applied. The oil and aluminum. chloride may be fed separately or previously mixed and fed to the chamber through a suitable inlet opening, such for instance as a manhole 17 in the cover. The bottom isprovided with a drain 18 through which the oil or tarry matters may be withdrawn and adjacent'to the bot-tom is a manhole 19 for cleaning purposes. The chamberv-may also'be provided with an inlet 20 forvoilor oil and aluminum chloride mixtures.

If the apparatus is to be used in connection with a heat treatment, suitable means are provided for heating the chamber, in which case it may serve as a still. As illustrated the chamber is mounted over a furnace 21. Although it is ordinarily desirable that-means be provided for-delivering to the heaters the solid matter which settles out at the bottom, this is particularly desirable where the heat treatment is employed. Asshown, I provide a lifting mechanism 22 in the form of a screw propeller closely adjacent to the bottom for causing an upward' circulation of the solid matter into the path of the beater. This propeller or litter is shown as being mounted on a vertical shaft 23, and the latter is driven by suitable gearing 24 from the shaft 12. f

In connection with the still there is provided a filter and condensing chamber in which there are one or more filter beds 25.

These may be madeof aluminum chloride or a mixture of some inertmaterial, such for instance as fullers earth and aluminum chloride, so as to render the filter beds more porous and facilitate their operation, .or there may be little or no aluminum chloride in the filter bed as installed, and the desired aluminum chloride be merely that which is brought over with the oil vapors from the still and condensed on or in the filter bed. Such accumulated aluminum chloride on the filter bed maybe scraped off and either with or without purification returned to the still. Above the filter bed is a receiving chamber 26 which is connected to the upper part of the still by a conduit 27, and

below the filter bed is a chamber 28 in which the mineral oil in liquid or vapor state collects after passing through the filter bed. Preferably the liquid level is kept below the filter bed. -The conduit 27 connecting the still and the filter is provided with a steam jacket 29 or other suitable heating means by which this conduit can be maintained at a temperature above the vaporizing point of aluminum chloride, that is, at or above 365 F., so that no aluminum chloride will condense and accumulate in this passage. The filter bed is provided with a jacket 30 having one or more inlets 31 and outlets 32 for a fluid which will maintain the filter bed at a temperature below 365 F. As it is preferable to condense the hydrocarbon at the same time the aluminum chloride is con-' densed, I may circulate cooling water in this jacket and maintain the filter bed at a comparatively low temperature.

The mineral oil and aluminum chloride are heated in the still 10 to the boiling point of the mixture or to such temperature as will cause the rapid evolution of vapors while the beating action is carried on. The resulting vapors of the oil will pass through the conduit 27 .to the condensing and filtering chamber, and there pass throughthe aluminum chloride of the filter bed 25. It will be noted that this filter bed is maintained substantially free of thetarry matters which are drawn out of the oil by the aluminum chloride in the still. If the temperature of the oil in the still necessary to maintain evolution of vapors rises above 365 F., as will be the ease in the treatment of some oils, the vapors as they reach the still outlet may not be above 365 F., but if they are, some of the aluminum chloride will pass over with the vapors of the oil and will condense in the chamber 26, where in its condensed form it acts on further vapors coming over from the still.

The operation in the still may be a continuous one with fresh oil and aluminum desired point in the still, or even until substantially all of the oil is vaporized and only the tarry or cokey mass remains behind. The process may be carried on at substantially atmospheric pressure in the still, .or a back pressure may be maintained by the resistance-of the filter bed, or a closure in the outlet from the chamber 28, or the pres- Y sur'e may be maintained below atmospheric pressure bythe application of suction or a partial vacuum to the outlet.

The same apparatus may be used for cold treatment of hydrocarbons in which case ,the beating apparatus is actuated, but with no fire 1n the still there will be no vaporization and only the intimate contact of the aluminum chloride with the oil so as to improve the color, odor and saturation. After a prelimmary treatment at room temperature the beater may be stopped, the solids permitted to settle, and. drawn off through the drain 18 to thereby remove the tarry matter from contact with the remaining oil, and thereafter fresh aluminum chloride may be added which will act in the absence of tarry matters, and will have materially greater effect in increasing the condition of saturation of the molecules. a

I have illustrated one form of beater or disrupting mechanism in Fig. 1, but ob.vi-- ously I do not desire to be restricted to this particular form. In Fig. GI ihave shown a modification inwhich there are aplurality of heaters similar to that illustrated in Fig. 1, but of smaller-size and operating to produce a variety of'cross currents in the liquid, and a largernumber of beating. or disrupting edges. My device as shown in Figure 6 will be operated by a chain of interlocking.

gears in the well known manner or by a belt from the source of power to a belt pulley of J, I

'each pair of beaters as in the belt pulley 16 of Figure 1.

Hereinbefore hydrous aluminum chloride as the agent employed for effecting the refining or purifying action as well as reduction in the boiling point of'the constituents. Certain other chlorides, such for instance as ferric chloride, might be employed, but less efiectively.

By means of my improved process the molecular contacting action which takes Ihave referred to only anplace after the separation of the tarry mat- I ters separates out certain oily, highly carbonaceous compounds which also assemble about the particles of aluminum chloride as nuclei, but 'these compounds thrown out in the second stage are not as resinous or pasty as those thrown out in the first stage, and the aluminum chloride is more easily recovered therefrom.-

I-have designated as solids all of the matters which settle out due" to their insoluble or immiscible character even though they be tarry, pasty, or semi liquid, and the term solid as used herein is to be so understood.

Although I have referred to the circulation of water in the jacket of the filter bed to keep down the temperature of the latter, it will be apparent-that other cooling mediums' might be employed which would merely maintain volatilization point of the aluminum chlothe temperature below the ride. Preferably the jacket is kept at as low a temperature as possible, so as to condense the very light products which otherwise mightpass oif as gases.

My improved process is more economical than any other with which I am familiar and resultsin a decolorizing, deodorizing and saturating action at less cost and m shorter time. In the heating treatment modification of the invention, no care need be exercised to maintain the still at any particular temperature other than that at which vapors are readily evolved.

Having thus described my invention, what I claim as new and desire to secure by Letters Patent is o .1. An apparatus for treatment of mineral oils including a still adapted to receive the oil to be treated and aluminum chloride,

means for heating-said still to a temperature at which vapors are evolved, means closely adjacent to the bottom of said still for causing an upward circulation of sohd matters settling to the bottom, and separate'beatcr mechanism above said upward circulating said solid matter,

means for breaking up filter bed therein,

the still to the filter bed, and.

from said still I means for maintaining the temperature of the filter bed belowthe volatilizing point of aluminum chloride.

2. An apparatus for the treatment of mineral oils including a chamber, mechanism therein closely adjacent to the bottom for re moving from the bottom solid matter settled thereon and forcing said solid matter upwardly, and separate beater mechanism above the first mentioned mechanism and within said chamber-for breaking u said solid matter, comprising a plurality 0 pairs of inter-rotating beater members rotatable about spaced parallel vertical axes.

3. An apparatus for the treatment of mineral oils, including a still adapted to receive mineral oil and aluminum chloride, means for heating the bottom of said still, a rotatable member closely adjacent to the bottom and acting to remove solid matter from the bottom and induce upward .currents in the oil to carry said'solid matter up from the bottom, and a pair of inter-rotating beater members above said first mentioned member for breaking up the solid matter raised by said first mentioned member, a condenser having a filter bed therein, means vapors from said still to said filter bed, means for maintaining the temperature of the vapors above the volatilizing point of aluminum chloride while passing from the still to a vapor bed and for conducting means for maintaining the temperature of the filter bed below the volatilizing point of aluminum chloride.

4. An apparatus for the treatment of mineral oils, including a still adapted to receive mineral oil and aluminum chloride, means for heating the bottom of said still, a rotatable member closely adjacent to the bottom and acting to remove solid matter from the bottom and induce upward currents in the oil to carry said solid matter up from the bottom, and a pair of inter-rotating beater members-in said chamber above said first mentioned member, and rotatable about spaced parallel vertical axes for breaking up the solid matter brought into the path of said beater members by said first mentioned member.

Signed at New York in the county of New York and State of New York this 22nd day ofcNovember A. D. 1922.

WILLIAM F. DOWNS. 

